纺织学报 ›› 2010, Vol. 31 ›› Issue (2): 73-76.

• 染整与化学品 • 上一篇    下一篇

基于气相色谱-离子阱法的纺织品及皮革中的富马酸二甲酯检测

孙忠松;王境堂;高永刚;蔡发   

  • 收稿日期:2009-01-20 修回日期:2009-05-31 出版日期:2010-02-15 发布日期:2010-02-15

Determination of dimethyl fumarate in textiles and leather products by Gas Chromatography-Ion Trap mass spectrometry

SUN Zhong-song;Wang Jing-tang;GAO Yong-gang;CAI Fa   

  • Received:2009-01-20 Revised:2009-05-31 Online:2010-02-15 Published:2010-02-15

摘要:

为了解决样品基体复杂,干扰测定的难题,建立了一种基于气相色谱-离子阱二级质谱(GC-MS/MS)检侧纺织品及皮革制品中富马酸二甲酯的方法。样品中富马酸二甲酯经乙腈提取,PSA/SAX小柱净化,GC-MS/MS进行定量和定性分析。该法采用化学源电离,甲醇作为反应气,并对前处理过程所用提取溶剂、净化过程,CID电压进行了优化,大大提高灵敏度和选择性。该方法在0.05-10.0μg/mL浓度范围内呈线性关系,相关系数为0.9998,仪器定量检出限LOQ为0.05mg/kg ,外标法定量。在50,500,1000μg/kg 3个水平的相对标准偏差为3.52%~6.12%,回收率为84.0%~99.5%。结果表明,相对于GC、GC-MS方法,GC-MS/MS分析时间短、无杂质峰干扰、灵敏度高,可以满足纺织品及皮革制品中检测大批量筛选要求。

Abstract:

To solve the interference of complex matrix sample, determination method of Dimethyl Fumarate in textiles and leather products was established based on Gas Chromatography-Ion Trap mass spectrometry. Dimethyl Fumarate in sample was extracted with acetonitrile and purified by the Supleco PSA/SAX SPE column, and then qualitative and qualitative analyses were performed by the GC-MS/MS. Chemical ionization mode was selected with methanol as reagent gas, and the extraction solvent,purification and CID voltage used in the pretreatment were optimized. Threrfore, sensitivity and selectivity were greatly improved. Linearity between the peak area and concentration of dimethyl fumarate was obtained in the range of 0.05-10.0μg/mL (r=0.9998),with its detection limit (LOQ) of 0.05mg/kg. External standard method was used in the quantitative analysis. Precision and recovery were tested by adding the standard dimethyl fumarate of 3 different concentration levels (50, 500, 1000μg/kg) to the leather samples, and analyzed by the proposed method, values of RSD (n=9) and recovery found were in the range of 3.52%-6.12% and 84.0%-99.5% respectively. The results showed that the proposed method was more sensitive and rapid, and no interference when compared with GC and GC-MS method. It can meet the analysis requirements of textile and leather samples in batches.

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